摘要
目的建立可同时检测辅助降血糖类保健食品中伏格列波糖、阿卡波糖、沙格列汀、阿格列汀、西格列汀、利格列汀和瑞格列汀的高效液相色谱串联高分辨质谱(HPLC-HRMS)分析方法。方法4种不同基质样品经甲醇超声提取后,采用CORTECS T3色谱柱(2.1 mm×100 mm,2.7μm),以0.1%甲酸水溶液-乙腈为流动相,梯度洗脱,柱温30℃,流速为0.3 ml/min,进样量5μl。采用离子阱质谱为检测器,电喷雾化正离子模式,以平行反应监测方式(PRM)进行检测。结果伏格列波糖、阿卡波糖和利格列汀在20~300μg/L范围内线性关系良好,定量限为1.00 mg/kg;在1.0,2.0,10.0 mg/kg加标水平下,回收率为80.2%~114.3%,相对标准偏差为0.2%~11.8%。沙格列汀、阿格列汀、西格列汀和瑞格列汀在2~30μg/L范围内线性关系良好,定量限为0.10 mg/kg;在0.1,0.2,1.0 mg/kg加标水平下,回收率为80.0%~112.8%,相对标准偏差为0.3%~9.0%。结论该方法高效、准确、简便,可用于辅助降血糖类保健食品中非法添加化合物的确证及定量测定。
Objective To establish a method for simultaneous determination of voglibose,acarbose,saxagliptin,alogliptin,sitagliptin,ligagliptin and repagliptin in auxiliary hypoglycemic health food by high performance liquid chromatography-high resolution mass spectrometry(HPLC-HRMS).Methods Four samples of different matrix were extracted with methanol by ultrasonic processing.The samples were separated on a CORTECS T3 column(2.1 mm×100 mm,2.7μm)with 0.1%formic acid solution-acetonitrile as mobile phase of gradient elution.The column temperature was 30℃,the flow rate was 0.3 ml/min,and the injection volume was 5μl.The ion trap mass spectrometer was used as the detector,and electrospray positive ion mode and parallel reaction monitoring(PRM)mode was used for detection.Results There were good linear relationships for voglibose,acarbose and ligagliptin in the range of 20-300μg/L,and the limit of quantification was 1.00 mg/kg.The recoveries were 80.2%-114.3%at the spiked levels of 1.0,2.0,10.0 mg/kg,with RSDs of 0.2%-11.8%.There were good linear relationships for saxagliptin,alogliptin,sitagliptin and repagliptin in the range of 2-30μg/L,and the limit of quantification was 0.10 mg/kg.The recoveries were 80.0%-112.8%at the spiked levels of 0.1,0.2,1.0 mg/kg,with RSDs of 0.3%-9.0%.Conclusion The method is efficient,accurate and simple,and can be used for the identification and quantitative determination of illegally added chemicals in auxiliary hypoglycemic health food.
作者
杨俊召
王婧娟
赵丽红
任静
董培智
YANG Jun-zhao;WANG Jing-juan;ZHAO Li-hong;REN Jing;DONG Pei-zhi(Shanxi Provincial Inspection and Testing Center,Key Laboratory of Food and Drug Safety Prevention and Control in Shanxi Province,Taiyuan 030031,China)
出处
《食品与药品》
2025年第1期24-30,共7页
Food and Drug
基金
食品药品安全防控山西省重点实验室基金项目资助(编号:202204010931006)。
作者简介
杨俊召,硕士,工程师,研究方向:食品药品质量检测,E-maill:yjzs1986@126.com;通信作者:董培智,博士,主任药师,研究方向:食品药品质量控制及标准研究,E-maill:peizhid@126.com。
